JPH07209164A - Method and device for identifying voltage compound and measuring concentration - Google Patents
Method and device for identifying voltage compound and measuring concentrationInfo
- Publication number
- JPH07209164A JPH07209164A JP1393294A JP1393294A JPH07209164A JP H07209164 A JPH07209164 A JP H07209164A JP 1393294 A JP1393294 A JP 1393294A JP 1393294 A JP1393294 A JP 1393294A JP H07209164 A JPH07209164 A JP H07209164A
- Authority
- JP
- Japan
- Prior art keywords
- volatile compound
- concentration
- sensor
- sample tube
- resonance frequency
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、試料中の揮発性化合物
を識別すると共に、揮発性化合物の濃度を測定する方法
および装置に関する。FIELD OF THE INVENTION The present invention relates to a method and apparatus for identifying volatile compounds in a sample and measuring the concentration of the volatile compounds.
【0002】[0002]
【従来の技術】生体では、多数の特性の異なる受容器、
すなわち嗅細胞からの応答パターンをパターン認識する
ことにより匂いを識別していると言われている。このよ
うな生体嗅覚機構を模擬した人工的な匂いの識別装置が
提案されている(特開平1−244335号公報)。こ
こで提案された匂い識別装置は、所定の匂いを呈する物
質に対して相互に異なる感受性を示す複数種類の受容体
を組み合わせた場合、この感受性の相違に由来して得ら
れる検出情報は、受容体毎に異なり、全体としては一定
のパターンを示すことに着目して開発された装置であ
る。BACKGROUND OF THE INVENTION In living organisms, there are many receptors with different characteristics,
That is, it is said that the odor is identified by recognizing the response pattern from the olfactory cell. An artificial odor discriminating device simulating such a biological olfactory mechanism has been proposed (JP-A-1-244335). The odor identification device proposed here is a combination of a plurality of types of receptors that exhibit different sensitivities to substances exhibiting a predetermined odor. This device was developed with a focus on showing a certain pattern as a whole, which is different for each body.
【0003】図2は、匂いのパターン認識により匂いを
識別する匂い識別装置を示すブロック図である。14
は、気体サンプルをセンサセルに送り込むためのキャリ
ヤガスの貯槽である。キャリヤガスとしては、一般に空
気が使用される。15は、キャリヤガスの流量を制御す
るためのマスフローコントローラである。17、18お
よび19は自動制御バルブである。バルブ19は、キャ
リヤガスのバイパス手段として設けられたものであり、
キャリヤガスをセンサセル10に送り込むときに開放さ
れ、バルブ17および18が開放されているときには閉
じるように制御される。バルブ17および18が開放さ
れると、キャリヤガスは送入用ニードル22を経て、試
料管21内に送入され、ついで試料管中のサンプル蒸気
と共に回収用ニードル23を経てセンサセル10に送入
される。センサセル10は、複数個の水晶振動子センサ
10a、10b、…、10hを収容している。水晶振動
子センサは、特開平1−244335号公報に開示され
ているものである。水晶振動子センサは、水晶振動子の
両面に設けた電極上にβ−シクロデキストリン等を塗布
して作製した。水晶振動子の両面に設けた電極は、コル
ビッツ型発振回路12の各発振回路に接続される。水晶
振動子センサ10a、10b、…、10hが8個である
ときは、それぞれがコルビッツ型発振回路12の各回路
に接続される。各回路の発振出力は、それぞれが8チャ
ンネルの周波数カウンタ13の各チャンネルに入力す
る。この周波数カウンタ13は、各水晶振動子センサの
周波数変化を同時に並列測定し、例えば1秒間隔でサン
プリングを行う。コンピュータ11は、検出された複
数、上記では8個、の電気信号の組合わせをパターン処
理することで、匂いを識別する。FIG. 2 is a block diagram showing an odor identifying device for identifying an odor by odor pattern recognition. 14
Is a reservoir of carrier gas for delivering the gas sample to the sensor cell. Air is generally used as the carrier gas. Reference numeral 15 is a mass flow controller for controlling the flow rate of the carrier gas. 17, 18 and 19 are automatic control valves. The valve 19 is provided as a bypass means for the carrier gas,
It is controlled to be opened when the carrier gas is sent to the sensor cell 10 and closed when the valves 17 and 18 are opened. When the valves 17 and 18 are opened, the carrier gas is introduced into the sample tube 21 through the injecting needle 22, and is then introduced into the sensor cell 10 through the collecting needle 23 together with the sample vapor in the sample tube. It The sensor cell 10 houses a plurality of crystal oscillator sensors 10a, 10b, ..., 10h. The crystal oscillator sensor is disclosed in JP-A-1-244335. The crystal oscillator sensor was produced by applying β-cyclodextrin or the like on the electrodes provided on both sides of the crystal oscillator. The electrodes provided on both sides of the crystal oscillator are connected to the respective oscillation circuits of the Kollwitz type oscillation circuit 12. When the number of the crystal oscillator sensors 10a, 10b, ..., 10h is eight, each of them is connected to each circuit of the Kolwitz type oscillation circuit 12. The oscillation output of each circuit is input to each channel of the 8-channel frequency counter 13. The frequency counter 13 simultaneously measures the frequency change of each crystal oscillator sensor in parallel and performs sampling, for example, at an interval of 1 second. The computer 11 identifies the odor by patterning the combination of the detected plurality of electric signals, eight in the above.
【0004】上記装置においては、液体状の匂い物質を
試料管の底部に入れ、そこから揮発性の匂い物質を揮発
化し、これを複数の水晶振動子センサで把握した周波数
変化をパターンとして認識し、匂いの種類を識別してい
る。このため試料中の各揮発性化合物の濃度を測定する
ことは極めて困難である。液体試料中の各揮発性化合物
が、気体として採取されるときに、液体中の各揮発性化
合物の濃度と平衡した濃度になっているか否かが不明で
あることによる。In the above apparatus, a liquid odorant is put in the bottom of the sample tube, and the volatile odorant is volatilized from the bottom, and the frequency change recognized by a plurality of quartz oscillator sensors is recognized as a pattern. , Identify the type of odor. Therefore, it is extremely difficult to measure the concentration of each volatile compound in the sample. This is because it is unclear whether or not each volatile compound in the liquid sample has a concentration in equilibrium with the concentration of each volatile compound in the liquid when collected as a gas.
【0005】試料中の揮発性化合物の濃度を測定する方
法としては、図3に示す装置を用いた方法が提案されて
いる。この装置について次に説明する。恒温槽30内に
試料管31を設置する。試料管31の内部にリード線3
7を介して発信回路36に接続された水晶振動子センサ
32を設置する。試料管31の口部は栓34(例えばテ
フロン製)で密封し、栓34には試料注入口33を設け
る。水晶振動子センサ32は、ATカットの水晶板の両
面に電極が設置され、この電極に感応膜が塗布されてい
る。この感応膜に匂い分子が吸着すると、質量負荷効果
により共振周波数が減少し、また脱着すると共振周波数
がもとに戻るという特性を有している。試料管31に予
め種類が判明している揮発性化合物を、該揮発性化合物
の平衡蒸気圧以下の濃度となるように注入し、水晶振動
子センサにより、共振周波数の変化を測定する。この変
化を予め求めておいた検量線と照合することにより揮発
性化合物の濃度を求めることができる。なお、図中35
は温度計を示す。しかし、この方法においては、試料と
しての揮発性化合物の種類を識別することができない。
また試料中に複数の揮発性化合物が混在しているときに
は、各揮発性化合物の濃度を求めることができない。As a method for measuring the concentration of volatile compounds in a sample, a method using the device shown in FIG. 3 has been proposed. This device will be described below. A sample tube 31 is installed in the constant temperature bath 30. Lead wire 3 inside the sample tube 31
The crystal oscillator sensor 32 connected to the transmitting circuit 36 via 7 is installed. The mouth of the sample tube 31 is sealed with a stopper 34 (made of Teflon, for example), and the stopper 34 is provided with a sample inlet 33. The crystal oscillator sensor 32 has electrodes on both sides of an AT-cut crystal plate, and a sensitive film is applied to the electrodes. When the odor molecules are adsorbed on the sensitive film, the resonance frequency is reduced due to the mass loading effect, and when desorbed, the resonance frequency is restored. A volatile compound of which the type is known in advance is injected into the sample tube 31 so that the concentration becomes equal to or lower than the equilibrium vapor pressure of the volatile compound, and the change in the resonance frequency is measured by the crystal oscillator sensor. The concentration of the volatile compound can be determined by collating this change with a calibration curve obtained in advance. In the figure, 35
Indicates a thermometer. However, this method cannot identify the type of volatile compound as a sample.
Further, when a plurality of volatile compounds are mixed in the sample, the concentration of each volatile compound cannot be obtained.
【0006】[0006]
【発明が解決しようとする課題】本発明は、揮発性化合
物の種類を識別できると共に該化合物の試料中の濃度を
測定できる方法および装置の提供を目的とする。さらに
はその種類が判明している揮発性化合物の混合物におい
て、各揮発性化合物の濃度を求めることができる測定方
法および装置の提供を目的とする。SUMMARY OF THE INVENTION It is an object of the present invention to provide a method and an apparatus capable of identifying the type of a volatile compound and measuring the concentration of the volatile compound in a sample. Furthermore, it is an object of the present invention to provide a measuring method and a device capable of determining the concentration of each volatile compound in a mixture of volatile compounds of which the types are known.
【0007】[0007]
【課題を解決するための手段】本発明は、電極面に揮発
性化合物の感応膜を被覆した複数個の水晶振動子センサ
を試料管中に挿入し、揮発性化合物の感応膜への吸着に
よる各水晶振動子の共振周波数の変化をパターン認識す
ることにより揮発性化合物を識別すると共に、複数個の
水晶振動子センサの共振周波数の変化を測定することに
より揮発性化合物の濃度を測定する方法を提供する。さ
らに本発明は、試料管と、複数個の水晶振動子センサと
を具備する揮発性化合物をパターン認識することで揮発
性化合物の種類を識別する揮発性化合物の識別装置にお
いて、該複数個の水晶振動子センサが該試料管内に備え
られていることを特徴とする揮発性化合物の識別および
/または濃度測定装置を提供する。SUMMARY OF THE INVENTION According to the present invention, a plurality of crystal oscillator sensors each having an electrode surface coated with a sensitive film of a volatile compound are inserted into a sample tube, and a volatile compound is adsorbed on the sensitive film. A method to identify the volatile compound by recognizing the change in the resonance frequency of each crystal oscillator and to measure the concentration of the volatile compound by measuring the change in the resonance frequency of multiple crystal oscillator sensors. provide. Furthermore, the present invention provides a volatile compound identification device for identifying the type of a volatile compound by pattern-recognizing a volatile compound, which comprises a sample tube and a plurality of crystal oscillator sensors. Provided is a device for identifying and / or measuring a concentration of a volatile compound, characterized in that a vibrator sensor is provided in the sample tube.
【0008】図1は本発明の揮発性化合物の識別および
/または濃度測定装置を示す説明図である。41は試料
管、42は水晶振動子センサ、43は水晶振動子センサ
と発振回路45とを接続するリード線、46は試料の注
入口、47は通気口、48は温度計を示す。発振回路4
5の後に設けられる周波数カウンタおよびコンピュータ
は図示を省略した。本発明の装置は、試料管41内部に
複数の水晶振動子センサ43を設けたところに特徴を有
する。水晶振動子センサに塗布される感応膜は、各水晶
振動子センサ毎に異なる。このため、揮発性化合物の感
応膜への吸着量が各感応膜毎に異なるので、各水晶振動
子センサ毎に共振周波数の減衰量が異なる。これにより
各水晶振動子センサの共振周波数の変化をパターンとし
て認識し、揮発性化合物の識別が可能となる。FIG. 1 is an explanatory view showing a device for identifying and / or measuring the concentration of volatile compounds of the present invention. 41 is a sample tube, 42 is a crystal oscillator sensor, 43 is a lead wire connecting the crystal oscillator sensor and the oscillation circuit 45, 46 is a sample inlet, 47 is a vent, and 48 is a thermometer. Oscillator circuit 4
The frequency counter and the computer provided after 5 are not shown. The apparatus of the present invention is characterized in that a plurality of crystal oscillator sensors 43 are provided inside the sample tube 41. The sensitive film applied to the crystal oscillator sensor is different for each crystal oscillator sensor. For this reason, since the adsorption amount of the volatile compound on the sensitive film is different for each sensitive film, the attenuation amount of the resonance frequency is different for each crystal oscillator sensor. As a result, the change in the resonance frequency of each crystal oscillator sensor is recognized as a pattern, and the volatile compound can be identified.
【0009】本発明においては、特定の揮発性化合物に
ついて、揮発性化合物の濃度と共振周波数の変化量との
間の関係を求めておく必要がある。このとき、揮発性化
合物の濃度は、測定温度の平衡蒸気圧以下の範囲から選
ぶ必要がある。試料管に注入すべき揮発性化合物の濃度
は、次式により算出されたCよりも低い濃度である。 C=[(22.4ρ・T・Vs)/(273M・V)]
×103 上式中の記号は次の意味をあらわす。 Cはサンプルの濃度(ppm) ρはサンプルの密
度(g/ml) Tは測定温度(°K) Vsはサンプルの
体積(μl) Mはサンプルの分子量 Vは試料管の体積
(l) 本発明によれば、複数の水晶振動子センサを用いること
により、揮発性化合物の種類を識別し、識別された揮発
性化合物について求められた検量線から濃度を求めるこ
とができる。試料中の揮発性化合物が混合物であるとき
には、この揮発性化合物の種類は予め同定しておく必要
がある。そしてこれらの揮発性化合物を予め各種の濃度
に混合した複数の試料を調整し、これらの試料について
周波数の変化パターンを求める。例えば水晶振動子セン
サが4個である場合には、4次元マトリックスであらわ
され、これを多変量解析の主成分分析法により、次元を
2次元に圧縮して散布図に表すことができる。揮発性化
合物の混合物についての周波数変化を上記と同様に処理
して散布図中における位置を求めることにより、各揮発
性化合物の濃度を求めることができる。In the present invention, it is necessary to obtain the relationship between the concentration of the volatile compound and the amount of change in the resonance frequency for the specific volatile compound. At this time, it is necessary to select the concentration of the volatile compound from the range below the equilibrium vapor pressure at the measurement temperature. The concentration of the volatile compound to be injected into the sample tube is lower than C calculated by the following equation. C = [(22.4ρ · T · Vs) / (273M · V)]
× 10 3 The symbols in the above formula have the following meanings. C is sample concentration (ppm) ρ is sample density (g / ml) T is measurement temperature (° K) Vs is sample volume (μl) M is sample molecular weight V is sample tube volume (l) According to this, by using a plurality of crystal oscillator sensors, the type of the volatile compound can be identified, and the concentration can be obtained from the calibration curve obtained for the identified volatile compound. When the volatile compound in the sample is a mixture, the type of the volatile compound needs to be identified in advance. Then, a plurality of samples in which these volatile compounds are mixed in various concentrations in advance are prepared, and a frequency change pattern is obtained for these samples. For example, when there are four quartz oscillator sensors, they are represented by a four-dimensional matrix, which can be compressed into two dimensions by the principal component analysis method of multivariate analysis and expressed in a scatter diagram. The concentration of each volatile compound can be determined by processing the frequency change of the mixture of volatile compounds in the same manner as above and determining the position in the scatter diagram.
【0010】[0010]
【発明の効果】本発明によれば、電極面に揮発性化合物
の感応膜を被覆した複数個の水晶振動子センサを試料管
中に挿入し、揮発性化合物の感応膜への吸着による各水
晶振動子の共振周波数の変化をパターン認識することに
より揮発性化合物の種類を識別すると共に、該揮発性化
合物について予め求められていた検量線から揮発性化合
物の濃度を測定する方法が提供される。さらに本発明に
よれば、試料管と、複数個の水晶振動子センサとを具備
する揮発性化合物をパターン認識することで揮発性化合
物の種類を識別する揮発性化合物の識別装置において、
該複数個の水晶振動子センサが該試料管内に備えられて
いることを特徴とする揮発性化合物の識別および/また
は濃度測定装置が提供される。以下実施例に基づいて本
発明をより詳細に説明する。According to the present invention, a plurality of quartz oscillator sensors each having an electrode surface coated with a sensitive film of a volatile compound are inserted into a sample tube, and each quartz crystal is obtained by adsorption of the volatile compound to the sensitive film. Provided is a method of identifying the type of a volatile compound by recognizing a change in the resonance frequency of a vibrator and measuring the concentration of the volatile compound from a calibration curve previously obtained for the volatile compound. Furthermore, according to the present invention, in a volatile compound identification device for identifying the type of a volatile compound by pattern-recognizing a volatile compound provided with a sample tube and a plurality of quartz oscillator sensors,
An apparatus for identifying and / or measuring a concentration of a volatile compound is provided, wherein the plurality of crystal oscillator sensors are provided in the sample tube. The present invention will be described in more detail based on the following examples.
【0011】実施例 図1に示す装置に下記に示す感応膜を塗布した水晶振動
子センサを用い、RoseOxide(C10H18O)およびCitron
ellal(C10H18O)の光学異性体について、検量線作成
結果を図4および図5に示す。なお、試料管内の温度は
28℃に保持し、水晶振動子としてはAT−CUTで基
本周波数10.3525MHzの市販品を用いた。EXAMPLE A crystal oscillator sensor having the following sensitive film applied to the device shown in FIG. 1 was used, and RoseOxide (C 10 H 18 O) and Citron were used.
The calibration curve preparation results for the ellal (C 10 H 18 O) optical isomers are shown in FIGS. 4 and 5. The temperature inside the sample tube was kept at 28 ° C., and a commercially available product of AT-CUT with a fundamental frequency of 10.32525 MHz was used as the crystal resonator.
【0012】 化合物名 組成式 分子量 Hexakis-(2,3,6-tri-O-Methyl)-α−Cyclodextrin C54H96O30 1224 Heptakis-(2,3,6-tri-O-Methyl)-β−Cyclodextrin C63H112O35 1428 Octakis-(2,3,6-tri-O-Methyl)-γ−Cyclodextrin C72H128O40 1632 Heptakis-(2,6-di-O-Methyl)-β−Cyclodextrin C56H98O35 1428 D体およびL体についてそれぞれ得られた検量線から、
D体およびL体の混合物について試料中の濃度を求める
ことができる。Compound name Compositional formula Molecular weight Hexakis- (2,3,6-tri-O-Methyl) -α-Cyclodextrin C 54 H 96 O 30 1224 Heptakis- (2,3,6-tri-O-Methyl)- β-Cyclodextrin C 63 H 112 O 35 1428 Octakis- (2,3,6-tri-O-Methyl) -γ-Cyclodextrin C 72 H 128 O 40 1632 Heptakis- (2,6-di-O-Methyl)- From the calibration curves obtained for β-Cyclodextrin C 56 H 98 O 35 1428 D-form and L-form,
The concentration in the sample can be determined for the mixture of D-form and L-form.
【図1】本発明の揮発性化合物の識別および濃度測定装
置を示す説明図である。FIG. 1 is an explanatory view showing a volatile compound identification and concentration measurement device of the present invention.
【図2】本発明の装置が適用される揮発性化合物識別装
置のフローチャートである。FIG. 2 is a flowchart of a volatile compound identification device to which the device of the present invention is applied.
【図3】水晶振動子センサを用いた濃度測定装置の説明
図である。FIG. 3 is an explanatory diagram of a concentration measuring device using a crystal oscillator sensor.
【図4】Rose Oxideに対する各感応膜の検量線を示すグ
ラフである。FIG. 4 is a graph showing a calibration curve of each sensitive film with respect to Rose Oxide.
【図5】Citronellalに対する各感応膜の検量線を示す
グラフであるFIG. 5 is a graph showing a calibration curve of each sensitive film for Citronellal.
41 試料管 42 水晶振動子センサ 45 発信回路 46 試料の注入口 41 sample tube 42 crystal oscillator sensor 45 oscillator circuit 46 sample inlet
Claims (2)
た複数個の水晶振動子センサを試料管中に挿入し、揮発
性化合物の感応膜への吸着による各水晶振動子の共振周
波数の変化をパターン認識することにより揮発性化合物
を識別すると共に、複数個の水晶振動子センサの共振周
波数の変化を測定することにより揮発性化合物の濃度を
測定する方法。1. A plurality of quartz oscillator sensors, each of which has an electrode surface coated with a sensitive film of a volatile compound, are inserted into a sample tube, and the resonance frequency of each quartz oscillator is detected by adsorption of the volatile compound to the sensitive film. A method of identifying a volatile compound by recognizing a change pattern and measuring a concentration of the volatile compound by measuring a change in resonance frequency of a plurality of crystal oscillator sensors.
を具備する揮発性化合物をパターン認識することで揮発
性化合物の種類を識別する揮発性化合物の識別装置にお
いて、該複数個の水晶振動子センサが該試料管内に備え
られていることを特徴とする揮発性化合物の識別および
/または濃度測定装置。2. A volatile compound identifying device for identifying the type of a volatile compound by pattern-recognizing a volatile compound, comprising a sample tube and a plurality of quartz oscillator sensors, A device for identifying and / or measuring a concentration of a volatile compound, characterized in that a vibrator sensor is provided in the sample tube.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP01393294A JP3302481B2 (en) | 1994-01-12 | 1994-01-12 | Method for identification and concentration measurement of volatile compounds |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP01393294A JP3302481B2 (en) | 1994-01-12 | 1994-01-12 | Method for identification and concentration measurement of volatile compounds |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH07209164A true JPH07209164A (en) | 1995-08-11 |
JP3302481B2 JP3302481B2 (en) | 2002-07-15 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP01393294A Expired - Lifetime JP3302481B2 (en) | 1994-01-12 | 1994-01-12 | Method for identification and concentration measurement of volatile compounds |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003532056A (en) * | 2000-04-05 | 2003-10-28 | ザ チャールズ スターク ドレイパー ラボラトリー インク | Apparatus and method for measuring mass of substance |
JP2007278830A (en) * | 2006-04-06 | 2007-10-25 | Ulvac Japan Ltd | Device and method for detecting food components |
JP2009031049A (en) * | 2007-07-25 | 2009-02-12 | Ulvac Japan Ltd | Evaluation method and evaluation device of optical isomer separability of chiral stationary phase for chromatography |
JP2009115760A (en) * | 2007-11-09 | 2009-05-28 | National Institute Of Advanced Industrial & Technology | Method and device for measuring concentration |
JP2010216851A (en) * | 2009-03-13 | 2010-09-30 | Olympus Corp | Substance detecting system |
JP2011117972A (en) * | 2011-02-14 | 2011-06-16 | Seiko Epson Corp | Vibrator, vibrator array, and electronic apparatus |
-
1994
- 1994-01-12 JP JP01393294A patent/JP3302481B2/en not_active Expired - Lifetime
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003532056A (en) * | 2000-04-05 | 2003-10-28 | ザ チャールズ スターク ドレイパー ラボラトリー インク | Apparatus and method for measuring mass of substance |
US7171844B2 (en) | 2000-04-05 | 2007-02-06 | The Charles Stark Draper Laboratory, Inc. | Apparatus and method for measuring the mass of a substance |
JP2007278830A (en) * | 2006-04-06 | 2007-10-25 | Ulvac Japan Ltd | Device and method for detecting food components |
JP2009031049A (en) * | 2007-07-25 | 2009-02-12 | Ulvac Japan Ltd | Evaluation method and evaluation device of optical isomer separability of chiral stationary phase for chromatography |
JP2009115760A (en) * | 2007-11-09 | 2009-05-28 | National Institute Of Advanced Industrial & Technology | Method and device for measuring concentration |
JP2010216851A (en) * | 2009-03-13 | 2010-09-30 | Olympus Corp | Substance detecting system |
JP2011117972A (en) * | 2011-02-14 | 2011-06-16 | Seiko Epson Corp | Vibrator, vibrator array, and electronic apparatus |
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